CN101983988B - Polyamide 6 composite and preparation method thereof - Google Patents
Polyamide 6 composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a reinforced and toughened polyamide 6 composite with good surface and a preparation method thereof. The composite comprises the following components by weight percent: 27-80% of high viscosity polyamide 6 resin, 5-20% of spinning grade polyamide 6 resin, 2-15% of elastomer flexibilizer, 5-60% of glass fiber and 0.5-5% of auxiliaries, wherein high viscosity polyamide 6 resin is used as the substrate to ensure the performances of the composite; spinning grade polyamide 6 resin is used as the fluidity improver which can increase the fluidity of the composite, reduce the content of the small-molecule gas and increase the surface gloss; the glass fiber covered by maleic anhydride grafted ethylene-octene copolymer can react with the amino end groups of polyamide 6 resin so as to increase the amount of resin covered on the surface of glass fiber and improve the binding ability of the surface of glass fiber and the resin substrate and all the mechanical properties of the material; and as the binding ability of glass fiber and resin is strong, the possibility that glass fiber migrates to the surface is reduced in the forming process and the smooth surface can be obtained.
Description
Technical field
The present invention relates to a kind of glass-fibre reinforced polyamide 6 materials, be specifically related to a kind of good surface and strengthen toughened polyamide 6 matrix materials and preparation method thereof.
Background technology
The polyamide 6 material is to use the most general material in the engineering plastics, is widely used in the industries such as automobile, building, electronic apparatus and household electrical appliances.Polyamide 6 can significantly improve its intensity, rigidity and toughness after glass fibre reinforced modified.Toughness reinforcing reinforced polyamide 6 matrix materials have good low-temperature flexibility, can be applied to power tool, office furniture, ski boot, cycle hub and other sports equipments etc.Because the requirement that outward appearance is used, these goods often need to have smooth surface, could be accepted by the human consumer.
Yet, having added a large amount of toughner in the resin glass fiber reinforcement technology polymeric amide PA6 matrix material, injection moulding product surface out is rough, and is floating fine serious, can not use at the high parts of some appearance requirement.In order to solve the floating fine problem that strengthens toughened polyamide PA6 matrix material, can improve by the method for adding inorganic mineral filler, such as number of patent application 200610118559.X (plasticizing enhancement nylon 6 composite material of a kind of good apparent mass and preparation method thereof), 200610064507.9 (a kind of modified nylon material with high smooth surface level and preparation method thereof).But interpolation inorganic mineral filler or reduction resin viscosity unavoidably cause the strength degradation of product, by the method that adds coupling agent the bonding force that improves resin and glass fibre are also affected to decline.Also improve the surface gloss of matrix material by adding amorphous polyamide or semiaromatic polyamide composition and multipolymer thereof, such as patent US5250604, US6958374, US6956081.It is higher to add this special polymeric amide cost, and performance is had certain influence.US5240974 and US5872175 adopt respectively organic silicon composite or phosphoric acid metalloid salt pair fiberglass surfacing to do special processing, and the bonding force of glass fibre and polyamide 6 strengthens after processing, and it is more functional to give material.This patent improves the surface that strengthens toughened polyamide 6 matrix materials by the grating of different viscosity resin and the special processing of glass fibre, has also improved intensity and the toughness of material simultaneously.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of simple, with low cost, the good surface that is applicable to scale of mass production strengthens toughened polyamide 6 matrix materials.
Another object of the present invention provides a kind of method that above-mentioned good surface strengthens toughened polyamide 6 matrix materials for preparing.
To achieve these goals, the present invention adopts following technical scheme:
A kind of good surface strengthens toughened polyamide 6 matrix materials, is comprised of the component of following weight percentage:
High bondable polyamide 6 resins 27～80%;
Spinning-grade polyamide 6 5～20%;
Elastic body toughening agent 2～15%;
Glass fibre 5～60%;
Auxiliary agent 0.5～5%.
Strengthen in toughened polyamide 6 matrix materials on above-mentioned good surface, described high bondable polyamide 6 resin viscosity scopes are preferably 2.6～3.4.
Strengthen in toughened polyamide 6 matrix materials on above-mentioned good surface, described spinning-grade polyamide 6, its principal character is that range of viscosities is 1.8～2.6, hot water extractables content is below 0.6%.
Strengthen in toughened polyamide 6 matrix materials on above-mentioned good surface, described elastic body toughening agent is preferably the ethylene-octene copolymer of maleic anhydride graft grafting.
Strengthen in toughened polyamide 6 matrix materials on above-mentioned good surface, described glass fibre is preferably compatilizer and coats the short glass fiber of processing; Described short fiber glass fibre is non-alkali glass, and the diameter of glass fibre is preferably 6～17 microns.
Strengthen in toughened polyamide 6 matrix materials on above-mentioned good surface, described compatilizer is preferably the ethylene-octene copolymer of maleic anhydride graft.
Strengthen in toughened polyamide 6 matrix materials on above-mentioned good surface, described auxiliary agent is one or more the mixture in lubricant, oxidation inhibitor, weather resisting agent, the nucleator.The adding of lubricant can form lubricant film at goods and mould product, has both improved release property and has also improved the product surface; The adding of nucleator can the refinement resin matrix crystal grain, improve the bonding force of resin matrix and fiberglass surfacing; The adding of oxidation inhibitor and weather resisting agent can reduce the degraded of material in the life-time service process aging, keeps the excellent surface of product.
Above-mentioned good surface strengthens toughened polyamide 6 composite manufacture methods, adopt the production of melt blending expressing technique, namely adopt the forcing machine that a side direction spout is arranged, add polyamide 6, elastic body toughening agent and other additive from main spout, the side spout adds short glass fiber; Behind the melt blending, through cooling, air-dry and granulation.
Compared with prior art, the present invention has following beneficial effect:
(1) high bondable polyamide 6 guarantees the performance of matrix material as the matrix of matrix material; The molecular weight of spinning-grade polyamide 6 is on the low side and narrow molecular weight distribution, can improve the mobile and stable of matrix material.But the hot water extractives content of spinning-grade polyamide 6 is lower, be lower than 0.6%, lower-molecular substance residual in the resin is described seldom, the micro-molecular gas that produces in forcing machine production and injection moulding machine injection moulding process is also corresponding lower, thereby reaches the effect of surperficial high gloss.Therefore, carry out grating with different viscosity and other polyamide 6 of level, kept good mechanical property, the enhancing toughened polyamide 6 material high comprehensive performances that obtain when improving flowability;
(2) glass fibre of processing through the ethylene-octene copolymer coating of maleic anhydride graft can react with the end amino of polyamide 6, increase resin in the coating on the surface of glass fibre, and improved glass surface and the binding ability of resin matrix and every mechanical property of material;
(3) because the binding ability of glass fibre and resin is strong, glass fibre reduces to the chance of surface transport in moulding process, thereby obtains smooth surface; The present invention is simple, and is with low cost, is applicable to scale of mass production.
Embodiment
Further explain the present invention below in conjunction with embodiment, but embodiment does not do any type of restriction to the present invention.
Following per-cent is weight percentage.
Embodiment 1
Adding 51.7% viscosity from main spout is that 2.8 polyamide 6,10% viscosity are 2.0 spinning-grade polyamide 6,7.5% maleic anhydride grafted ethene-octene copolymer, 0.5% phenolic antioxidant and 0.3% long-chain carboxylic acid's salt, adds 30% through coating the short glass fiber of processing from the side spout.Melt blending becomes pellet by cooling, air-dry, pelletizing in twin screw extruder.Pellet is injection molded into standard mechanics test bars and colour table is tested.
Embodiment 2
Adding 56.7% viscosity from main spout is that 2.8 polyamide 6,10% viscosity are 2.0 spinning-grade polyamide 6,7.5% maleic anhydride grafted ethene-octene copolymer, 0.5% phenolic antioxidant and 0.3% long-chain carboxylic acid's salt, adds 25% through coating the short glass fiber of processing from the side spout.Melt blending becomes pellet by cooling, air-dry, pelletizing in twin screw extruder.Pellet is injection molded into standard mechanics test bars and colour table is tested.
Embodiment 3
Adding 37.2% viscosity from main spout is that 2.8 polyamide 6,20% viscosity are 2.0 spinning-grade polyamide 6,12% maleic anhydride grafted ethene-octene copolymer, 0.5% phenolic antioxidant and 0.3% long-chain carboxylic acid's salt, adds 30% through coating the short glass fiber of processing from the side spout.Melt blending becomes pellet by cooling, air-dry, pelletizing in twin screw extruder.Pellet is injection molded into standard mechanics test bars and colour table is tested.
Embodiment 4
Adding 41.7% viscosity from main spout is that 2.8 polyamide 6,20% viscosity are 2.4 spinning-grade polyamide 6,7.5% maleic anhydride grafted ethene-octene copolymer, 0.5% phenolic antioxidant and 0.3% long-chain carboxylic acid's salt, adds 30% through coating the short glass fiber of processing from the side spout.Melt blending becomes pellet by cooling, air-dry, pelletizing in twin screw extruder.Pellet is injection molded into standard mechanics test bars and colour table is tested.
Embodiment 5
Adding 56.7% viscosity from main spout is that 2.8 polyamide 6,20% viscosity are 2.0 spinning-grade polyamide 6,7.5% maleic anhydride grafted ethene-octene copolymer, 0.5% phenolic antioxidant and 0.3% long-chain carboxylic acid's salt, adds 15% through coating the short glass fiber of processing from the side spout.Melt blending becomes pellet by cooling, air-dry, pelletizing in twin screw extruder.Pellet is injection molded into standard mechanics test bars and colour table is tested.
Embodiment 6
Adding 52.2% viscosity from main spout is that 3.0 polyamide 6,20% viscosity are 2.0 spinning-grade polyamide 6,12% maleic anhydride grafted ethene-octene copolymer, 0.5% phenolic antioxidant and 0.3% long-chain carboxylic acid's salt, adds 15% through coating the short glass fiber of processing from the side spout.Melt blending becomes pellet by cooling, air-dry, pelletizing in twin screw extruder.Pellet is injection molded into standard mechanics test bars and colour table is tested.
Embodiment 7
Adding 27% viscosity from main spout is that 2.8 polyamide 6,20% viscosity are 2.0 spinning-grade polyamide 6,2% maleic anhydride grafted ethene-octene copolymer, 0.5% phenolic antioxidant and 0.5% long-chain carboxylic acid's salt, adds 50% through coating the short glass fiber of processing from the side spout.Melt blending becomes pellet by cooling, air-dry, pelletizing in twin screw extruder.Pellet is injection molded into standard mechanics test bars and colour table is tested.
Embodiment 8
Adding 67.2% viscosity from main spout is that 3.0 polyamide 6,20% viscosity are 2.0 spinning-grade polyamide 6,2% maleic anhydride grafted ethene-octene copolymer, 0.5% phenolic antioxidant and 0.3% long-chain carboxylic acid's salt, adds 10% through coating the short glass fiber of processing from the side spout.Melt blending becomes pellet by cooling, air-dry, pelletizing in twin screw extruder.Pellet is injection molded into standard mechanics test bars and colour table is tested.
Comparative example 1
Be that to replace to viscosity be 2.0 polyamide 6 for 2.8 polyamide resin 6 fat equivalent with the viscosity among the embodiment 1, under other constant prerequisite, adopt the preparation of same process method to strengthen toughened polyamide 6 particulate material, then be injection molded into standard mechanics test bars and colour table and test.
Comparative example 2
With the viscosity among the embodiment 1 be 2.0 spinning-grade polyamide 6 equivalent to replace to viscosity be 2.5, but the hot water extractives content is 0.7% polyamide 6, maleic anhydride grafted ethene-octene copolymer adds 12% to.Under other constant prerequisite, adopt the preparation of same process method to strengthen toughened polyamide 6 particulate material, then be injection molded into standard mechanics test bars and colour table and test.
Comparative example 3
Be that 2.4 spinning-grade polyamide 6 equivalent replaces that to become viscosity be 2.4 with the viscosity among the embodiment 4, but the hot water extractives content is 0.8% polyamide 6.Under other constant prerequisite, adopt the preparation of same process method to strengthen toughened polyamide 6 particulate material, then be injection molded into standard mechanics test bars and colour table and test.
Comparative example 4
Change the short glass fiber through maleic anhydride grafted ethene-octene copolymer coating is processed among the embodiment 1 into undressed short glass fiber, under other constant prerequisite, adopt the preparation of same process method to strengthen toughened polyamide 6 particulate material, then be injection molded into standard mechanics test bars and colour table and test.
Comparative example 5
Change the short glass fiber through maleic anhydride grafted ethene-octene copolymer coating is processed among the embodiment 3 into short glass fiber that Silane coupling agent KH550 is processed, under other constant prerequisite, adopt the preparation of same process method to strengthen toughened polyamide 6 particulate material, then be injection molded into standard mechanics test bars and colour table and test.
Comparative example 6
Long-chain carboxylic acid's salt among the embodiment 1 is removed, under other constant prerequisite, adopt the preparation of same process method to strengthen toughened polyamide 6 particulate material, then be injection molded into standard mechanics test bars and colour table and test.
Performance evaluation criterion and index
Tensile property is tested by ISO 527-2, and rate of extension is 10mm/min.Bending property is tested by ISO 178, and rate of bending is 2mm/min.The socle girder impact property is tested according to ISO 180.Melt flow index is tested according to ISO 1133, and temperature is selected 260 ℃, and counterweight is 2.16KG.The colour table that the smooth surface situation is made according to equal injecting condition is according to the mirror surface luster at 60 ° of angles of GB 8807 mensuration.
From embodiment 1 and comparative example 1 contrast, all select the resin of viscosity lower (viscosity 2.0), mechanical property especially low temperature impact properties descends obviously.From embodiment 1 and comparative example 2 contrasts, and embodiment 4 finds out with comparative example 3 contrasts, but changes the spinning-grade polyamide 6 into the hot water extractives content greater than 0.6% polyamide 6, and the surface gloss of material descends obviously.
From embodiment 1 and comparative example 4 contrasts, the mechanical property of embodiment 1 comprises intensity and toughness all than comparative example 3 height, and the short glass fiber that this explanation process maleic anhydride graft is processed and the binding ability of resin matrix are stronger.Coat the glass fibre of processing through compatilizer and also have certain Efficient Adhesive Promotion, cause the flowability of embodiment 1 to reduce, so this also needs to add the flowability that low viscous spinning-grade polyamide 6 is adjusted material.Embodiment 3 and comparative example 5 contrasts, if after glass changed the silane coupling agent processing into, material property reduced obviously, and surface floating fiber is obvious, glossiness obviously reduces.
From embodiment 1 and comparative example 6 contrasts, remove other additives after, material flowability reduces obviously, and surface floating fiber is serious.
From embodiment 1 to 8, the content of glass fibre and toughner is higher, and the surface is poorer; The viscosity of spinning-grade polyamide 6 is lower, and ratio is higher, and the surface of material is just better.All in all, the surface gloss of embodiment 1 to 8 is generally more than 50, and the glossiness major part of comparative example is below 50.Therefore can and adjust by fill a prescription composite of the present invention according to different mechanical property requirements, make enhancing toughened polyamide 6 materials of smooth surface and good mechanical performance.
The present invention carries out grating with different viscosity and other polyamide 6 of level, coats the short glass fiber of processing by adding, and has improved the boundary strength of glass fibre and resin matrix, strengthens toughened polyamide 6 matrix materials thereby obtain good surface.
Table 1 has been listed the sample testing result of above-mentioned all embodiment and comparative example.
Claims (1)
1. a polyamide 6 composite material is characterized in that, is made according to corresponding preparation method by the component of following weight percentage:
Adding 51.7% viscosity from main spout is that 2.8 polyamide 6,10% viscosity are 2.0 spinning-grade polyamide 6,7.5% maleic anhydride grafted ethene-octene copolymer, 0.5% phenolic antioxidant and 0.3% long-chain carboxylic acid's salt, adds 30% through coating the short glass fiber of processing from the side spout; Melt blending becomes pellet by cooling, air-dry, pelletizing in twin screw extruder;
Or to add 56.7% viscosity from main spout be that 2.8 polyamide 6,10% viscosity are 2.0 spinning-grade polyamide 6,7.5% maleic anhydride grafted ethene-octene copolymer, 0.5% phenolic antioxidant and 0.3% long-chain carboxylic acid's salt, adds 25% through coating the short glass fiber of processing from the side spout; Melt blending becomes pellet by cooling, air-dry, pelletizing in twin screw extruder;
Or to add 37.2% viscosity from main spout be that 2.8 polyamide 6,20% viscosity are 2.0 spinning-grade polyamide 6,12% maleic anhydride grafted ethene-octene copolymer, 0.5% phenolic antioxidant and 0.3% long-chain carboxylic acid's salt, adds 30% through coating the short glass fiber of processing from the side spout; Melt blending becomes pellet by cooling, air-dry, pelletizing in twin screw extruder;
Or to add 41.7% viscosity from main spout be that 2.8 polyamide 6,20% viscosity are 2.4 spinning-grade polyamide 6,7.5% maleic anhydride grafted ethene-octene copolymer, 0.5% phenolic antioxidant and 0.3% long-chain carboxylic acid's salt, adds 30% through coating the short glass fiber of processing from the side spout; In twin screw extruder melting its mixed become pellet by cooling, air-dry, pelletizing;
Or to add 56.7% viscosity from main spout be that 2.8 polyamide 6,20% viscosity are 2.0 spinning-grade polyamide 6,7.5% maleic anhydride grafted ethene-octene copolymer, 0.5% phenolic antioxidant and 0.3% long-chain carboxylic acid's salt, adds 15% through coating the short glass fiber of processing from the side spout; Melt blending becomes pellet by cooling, air-dry, pelletizing in twin screw extruder;
Or to add 52.2% viscosity from main spout be that 3.0 polyamide 6,20% viscosity are 2.0 spinning-grade polyamide 6,12% maleic anhydride grafted ethene-octene copolymer, 0.5% phenolic antioxidant and 0.3% long-chain carboxylic acid's salt, adds 15% through coating the short glass fiber of processing from the side spout; Melt blending becomes pellet by cooling, air-dry, pelletizing in twin screw extruder;
Or to add 27% viscosity from main spout be that 2.8 polyamide 6,20% viscosity are 2.0 spinning-grade polyamide 6,2% maleic anhydride grafted ethene-octene copolymer, 0.5% phenolic antioxidant and 0.5% long-chain carboxylic acid's salt, adds 50% through coating the short glass fiber of processing from the side spout; Melt blending becomes pellet by cooling, air-dry, pelletizing in twin screw extruder;
Or to add 67.2% viscosity from main spout be that 3.0 polyamide 6,20% viscosity are 2.0 spinning-grade polyamide 6,2% maleic anhydride grafted ethene-octene copolymer, 0.5% phenolic antioxidant and 0.3% long-chain carboxylic acid's salt, adds 10% through coating the short glass fiber of processing from the side spout; Melt blending becomes pellet by cooling, air-dry, pelletizing in twin screw extruder.
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| CN116285325B (en) * | 2023-04-11 | 2024-01-30 | 丰汇新材料科技(湖州)有限公司 | Polyamide 6 composite material and preparation method thereof |
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